Dimethylformamide → 4-iodo-N-methyl-2-nitroaniline

HRID 1477297노트

반응식

HRID 1477297 반응식
[I:1][C:2]1[CH:7]=[CH:6][C:5]([NH2:8])=[C:4]([N+:9]([O-:11])=[O:10])[CH:3]=1.[H-].[Na+].[CH3:14]N(C=O)C.IC>O>[I:1][C:2]1[CH:7]=[CH:6][C:5]([NH:8][CH3:14])=[C:4]([N+:9]([O-:11])=[O:10])[CH:3]=1

참가 물질

6

반응물 4

HCID 6228DimethylformamideHCID 6328Methyl iodideHCID 24758Sodium hydrideHCID 113690724-Iodo-2-nitroaniline

생성물 1

HCID 658098494-iodo-N-methyl-2-nitroaniline

시약·촉매·용매 1

HCID 962Water용매

실험 절차

To a mixture of 4-iodo-2-nitro-phenyl amine (2.0 g), 60% sodium hydride (oil) (330 mg), and DMF (20 ml) was added dropwise iodomethane (470 μL) while ice-cooling. The reaction mixture was heated to room temperature, and then stirred for 2 hours. To the reaction mixture was added water, and the mixture was extracted with ethyl acetate. The organic layer was dried over sodium sulfate, and concentrated under reduced pressure. The residue was subjected to silica gel column chromatography to give (4-iodo-2-nitro-phenyl)-methyl-amine (2.0 g).

후처리

  1. temperaturecooling
  2. extractionthe mixture was extracted with ethyl acetate
  3. dry with materialThe organic layer was dried over sodium sulfate
  4. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-2c0805152ed242489e6d04d81b2e34e2
출처 데이터셋
uspto-grants-2016_08
특허 번호
US09403771B2

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